反应详情

To 5.00 g of 3-(2,5-difluoro-4-nitrophenyl)-1-methyl-5-(trifluoromethyl)-1H-pyrazole dissolved in 50 ml of acetic acid was added 15 ml of sulfuryl chloride. The mixture was mildly refluxed with 2 ml portions of sulfuryl chloride added every 15 minutes. After 6 hours, the mixture was cooled, then diluted with water and extracted with ether. The ether was washed 3 times with water, dried with anhydrous magnesium sulfate, filtered and concentrated. The residue was chromatographed to give a quantitative yield of 4-chloro-3-(2,5-difluoro-4-nitrophenyl)-1-methyl-5-(trifluoromethyl)-1H-pyrazole.

1. additionadded every 15 minutes
2. temperaturethe mixture was cooled
3. extractionextracted with ether
4. washThe ether was washed 3 times with water
5. dry with materialdried with anhydrous magnesium sulfate
6. filtrationfiltered
7. concentrationconcentrated
8. customThe residue was chromatographed